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#$Date: 2022-09-15 01:26:15 +0300 (Thu, 15 Sep 2022) $
#$Revision: 277847 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/06/16/4061615.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4061615
loop_
_publ_author_name
'Oulié, Pascal'
'Bréfuel, Nicolas'
'Vendier, Laure'
'Duhayon, Carine'
'Etienne, Michel'
_publ_section_title
;
A New Way to Scorpionate Niobium Complexes: Terminal Alkyne,
Imido and Oxo Complexes, and the Rearrangement of a-Agostic
Ethyl Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4306
_journal_page_last               4314
_journal_paper_doi               10.1021/om050423f
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C24 H30 B1 Cl2 N6 Nb1'
_chemical_formula_sum            'C24 H30 B Cl2 N6 Nb'
_chemical_formula_weight         577.16
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                74.971(5)
_cell_angle_beta                 85.341(5)
_cell_angle_gamma                84.280(6)
_cell_formula_units_Z            2
_cell_length_a                   10.4566(8)
_cell_length_b                   11.1476(7)
_cell_length_c                   11.9708(6)
_cell_measurement_temperature    180(2)
_cell_measurement_wavelength     0.71073
_cell_volume                     1338.72(15)
_diffrn_ambient_temperature      180
_exptl_crystal_density_diffrn    1.432
_cod_database_code               4061615
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.49196(18) 0.19991(19) 0.31036(17) 0.0243(4) Uani 1 1 d . . .
H1 H 0.4309 0.1513 0.3609 0.029 Uiso 1 1 calc R . .
C2 C 0.51190(17) 0.31045(18) 0.24665(17) 0.0236(4) Uani 1 1 d . . .
C3 C 0.4610(2) 0.4422(2) 0.2041(2) 0.0373(5) Uani 1 1 d . . .
H3A H 0.4507 0.4596 0.1198 0.045 Uiso 1 1 calc R . .
H3B H 0.5255 0.4966 0.2155 0.045 Uiso 1 1 calc R . .
C4 C 0.33403(19) 0.47672(17) 0.26210(18) 0.0260(4) Uani 1 1 d . . .
C5 C 0.3280(3) 0.5206(3) 0.3607(2) 0.0446(6) Uani 1 1 d . . .
H5 H 0.4054 0.529 0.3933 0.054 Uiso 1 1 calc R . .
C6 C 0.2092(3) 0.5528(3) 0.4128(2) 0.0484(6) Uani 1 1 d . . .
H6 H 0.2061 0.5817 0.4811 0.058 Uiso 1 1 calc R . .
C7 C 0.0979(2) 0.5425(2) 0.3649(2) 0.0404(6) Uani 1 1 d . . .
H7 H 0.0173 0.566 0.3991 0.048 Uiso 1 1 calc R . .
C8 C 0.1018(2) 0.4984(2) 0.2678(2) 0.0377(5) Uani 1 1 d . . .
H8 H 0.0241 0.4901 0.2356 0.045 Uiso 1 1 calc R . .
C9 C 0.2191(2) 0.4661(2) 0.2169(2) 0.0318(4) Uani 1 1 d . . .
H9 H 0.2209 0.4359 0.1495 0.038 Uiso 1 1 calc R . .
C11 C 0.42238(19) 0.0492(2) 0.12771(19) 0.0292(4) Uani 1 1 d . . .
H11A H 0.3702 0.0713 0.1924 0.044 Uiso 1 1 calc R . .
H11B H 0.3712 0.0051 0.0886 0.044 Uiso 1 1 calc R . .
H11C H 0.4495 0.1252 0.0727 0.044 Uiso 1 1 calc R . .
C12 C 0.53850(18) -0.03306(18) 0.17273(16) 0.0216(4) Uani 1 1 d . . .
C13 C 0.5635(2) -0.15975(19) 0.18040(18) 0.0271(4) Uani 1 1 d . . .
H13 H 0.5098 -0.2121 0.1576 0.033 Uiso 1 1 calc R . .
C14 C 0.6817(2) -0.19426(18) 0.22757(18) 0.0254(4) Uani 1 1 d . . .
C15 C 0.7545(3) -0.3195(2) 0.2550(3) 0.0447(6) Uani 1 1 d . . .
H15A H 0.8417 -0.3128 0.2184 0.067 Uiso 1 1 calc R . .
H15B H 0.7103 -0.3774 0.2255 0.067 Uiso 1 1 calc R . .
H15C H 0.7594 -0.3504 0.3391 0.067 Uiso 1 1 calc R . .
C21 C 0.6214(2) 0.1810(2) 0.54720(19) 0.0359(5) Uani 1 1 d . . .
H21A H 0.6262 0.26 0.488 0.054 Uiso 1 1 calc R . .
H21B H 0.6433 0.1919 0.6218 0.054 Uiso 1 1 calc R . .
H21C H 0.5338 0.1546 0.5541 0.054 Uiso 1 1 calc R . .
C22 C 0.71374(19) 0.08405(19) 0.51323(16) 0.0243(4) Uani 1 1 d . . .
C23 C 0.7900(2) -0.0092(2) 0.58513(16) 0.0275(4) Uani 1 1 d . . .
H23 H 0.7958 -0.0221 0.6662 0.033 Uiso 1 1 calc R . .
C24 C 0.85544(18) -0.07939(18) 0.51616(16) 0.0234(4) Uani 1 1 d . . .
C25 C 0.9478(2) -0.1916(2) 0.5501(2) 0.0351(5) Uani 1 1 d . . .
H25A H 0.9085 -0.2652 0.5427 0.053 Uiso 1 1 calc R . .
H25B H 0.9693 -0.2032 0.6306 0.053 Uiso 1 1 calc R . .
H25C H 1.0264 -0.1802 0.4993 0.053 Uiso 1 1 calc R . .
C31 C 0.9655(2) 0.33093(18) 0.04085(18) 0.0280(4) Uani 1 1 d . . .
H31A H 0.8998 0.3489 -0.0164 0.042 Uiso 1 1 calc R . .
H31B H 1.0485 0.3555 0.002 0.042 Uiso 1 1 calc R . .
H31C H 0.941 0.3779 0.0992 0.042 Uiso 1 1 calc R . .
C32 C 0.97648(17) 0.19462(17) 0.09839(15) 0.0201(3) Uani 1 1 d . . .
C33 C 1.07764(17) 0.10834(18) 0.08209(17) 0.0227(4) Uani 1 1 d . . .
H33 H 1.1532 0.1246 0.0327 0.027 Uiso 1 1 calc R . .
C34 C 1.04610(17) -0.00554(17) 0.15206(16) 0.0202(3) Uani 1 1 d . . .
C35 C 1.1184(2) -0.13118(19) 0.1681(2) 0.0292(4) Uani 1 1 d . . .
H35A H 1.1556 -0.1553 0.2441 0.044 Uiso 1 1 calc R . .
H35B H 1.1874 -0.1279 0.1072 0.044 Uiso 1 1 calc R . .
H35C H 1.0594 -0.1926 0.1636 0.044 Uiso 1 1 calc R . .
N1 N 0.63890(14) 0.00859(14) 0.21281(13) 0.0178(3) Uani 1 1 d . . .
N2 N 0.72623(14) -0.09208(14) 0.24649(13) 0.0187(3) Uani 1 1 d . . .
N3 N 0.73346(15) 0.07240(14) 0.40311(13) 0.0196(3) Uani 1 1 d . . .
N4 N 0.82048(14) -0.02959(14) 0.40661(13) 0.0189(3) Uani 1 1 d . . .
N5 N 0.88651(14) 0.13688(13) 0.17440(13) 0.0174(3) Uani 1 1 d . . .
N6 N 0.93167(14) 0.01350(13) 0.20761(13) 0.0175(3) Uani 1 1 d . . .
Cl1 Cl 0.65027(4) 0.27254(5) 0.02841(4) 0.02558(10) Uani 1 1 d . . .
Cl2 Cl 0.77799(4) 0.35568(4) 0.28646(4) 0.02503(10) Uani 1 1 d . . .
Nb1 Nb 0.677118(14) 0.195396(14) 0.232827(13) 0.01597(6) Uani 1 1 d . . .
B1 B 0.85374(19) -0.07904(18) 0.29754(18) 0.0187(4) Uani 1 1 d . . .
H1A H 0.9042 -0.1619 0.3188 0.022 Uiso 1 1 calc R . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.297(3) . ?
C1 Nb1 2.0797(19) . ?
C1 H1 0.95 . ?
C2 C3 1.484(3) . ?
C2 Nb1 2.0686(18) . ?
C3 C4 1.510(3) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 C5 1.385(3) . ?
C4 C9 1.385(3) . ?
C5 C6 1.401(4) . ?
C5 H5 0.95 . ?
C6 C7 1.366(4) . ?
C6 H6 0.95 . ?
C7 C8 1.370(4) . ?
C7 H7 0.95 . ?
C8 C9 1.382(3) . ?
C8 H8 0.95 . ?
C9 H9 0.95 . ?
C11 C12 1.495(3) . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 N1 1.357(2) . ?
C12 C13 1.391(3) . ?
C13 C14 1.378(3) . ?
C13 H13 0.95 . ?
C14 N2 1.350(2) . ?
C14 C15 1.492(3) . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C15 H15C 0.98 . ?
C21 C22 1.491(3) . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 N3 1.355(2) . ?
C22 C23 1.393(3) . ?
C23 C24 1.377(3) . ?
C23 H23 0.95 . ?
C24 N4 1.350(2) . ?
C24 C25 1.491(3) . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C31 C32 1.494(3) . ?
C31 H31A 0.98 . ?
C31 H31B 0.98 . ?
C31 H31C 0.98 . ?
C32 N5 1.344(2) . ?
C32 C33 1.394(3) . ?
C33 C34 1.382(3) . ?
C33 H33 0.95 . ?
C34 N6 1.346(2) . ?
C34 C35 1.498(3) . ?
C35 H35A 0.98 . ?
C35 H35B 0.98 . ?
C35 H35C 0.98 . ?
N1 N2 1.370(2) . ?
N1 Nb1 2.2346(15) . ?
N2 B1 1.546(2) . ?
N3 N4 1.378(2) . ?
N3 Nb1 2.2286(15) . ?
N4 B1 1.546(3) . ?
N5 N6 1.375(2) . ?
N5 Nb1 2.3263(15) . ?
N6 B1 1.529(2) . ?
Cl1 Nb1 2.4039(5) . ?
Cl2 Nb1 2.4079(5) . ?
B1 H1A 1 . ?
